 
data_siloxy 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C16 H26 O5 S' 
_chemical_formula_weight          330.43 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.1246   0.1234 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            orthorhombic 
_symmetry_space_group_name_H-M    P212121 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 'x+1/2, -y+1/2, -z' 
 '-x, y+1/2, -z+1/2' 
 
_cell_length_a                    6.4313(1) 
_cell_length_b                    11.6244(1) 
_cell_length_c                    22.4048(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      1674.98(4) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     153(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        prisms 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.30 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.14 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.310 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              712 
_exptl_absorpt_coefficient_mu     0.214 
_exptl_absorpt_correction_type    none 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       153(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Nonius Kappa CCD' 
_diffrn_measurement_method        ω-scans 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             13670 
_diffrn_reflns_av_R_equivalents   0.1062 
_diffrn_reflns_av_sigmaI/netI     0.0714 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        8 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -29 
_diffrn_reflns_limit_l_max        28 
_diffrn_reflns_theta_min          3.30 
_diffrn_reflns_theta_max          27.50 
_reflns_number_total              3846 
_reflns_number_gt                 3623 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0799P)²+0.6254P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.13(11) 
_refine_ls_number_reflns          3846 
_refine_ls_number_parameters      200 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0566 
_refine_ls_R_factor_gt            0.0524 
_refine_ls_wR_factor_ref          0.1443 
_refine_ls_wR_factor_gt           0.1425 
_refine_ls_goodness_of_fit_ref    1.135 
_refine_ls_restrained_S_all       1.135 
_refine_ls_shift/su_max           0.003 
_refine_ls_shift/su_mean          0.001 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
SI1 S 0.24726(8) 0.23224(5) 0.34253(3) 0.02029(16) Uani 1 1 d . . . 
O2 O 0.4955(2) 0.21145(15) 0.35693(9) 0.0222(4) Uani 1 1 d . . . 
C3 C 0.5933(4) 0.1127(2) 0.38227(12) 0.0216(5) Uani 1 1 d . . . 
H3A H 0.6503 0.1314 0.4206 0.026 Uiso 1 1 d R . . 
H3B H 0.7050 0.0884 0.3568 0.026 Uiso 1 1 d R . . 
C4 C 0.4372(4) 0.0155(2) 0.38873(11) 0.0180(4) Uani 1 1 d . . . 
H4 H 0.4057 -0.0153 0.3500 0.022 Uiso 1 1 d R . . 
O5 O 0.5237(2) -0.07454(15) 0.42541(8) 0.0214(4) Uani 1 1 d . . . 
C6 C 0.4005(4) -0.1740(2) 0.41739(12) 0.0217(5) Uani 1 1 d . . . 
H6 H 0.4536 -0.2295 0.3896 0.026 Uiso 1 1 d R . . 
C7 C 0.2761(4) -0.2210(2) 0.46891(12) 0.0228(5) Uani 1 1 d . . . 
H7 H 0.2570 -0.3025 0.4731 0.027 Uiso 1 1 d R . . 
C8 C 0.2493(4) -0.14582(19) 0.52199(11) 0.0203(4) Uani 1 1 d . . . 
O9 O 0.1537(3) -0.04610(15) 0.50618(8) 0.0215(4) Uani 1 1 d . . . 
C10 C 0.1094(4) -0.0421(2) 0.44265(11) 0.0194(5) Uani 1 1 d . . . 
H10 H -0.0364 -0.0292 0.4363 0.023 Uiso 1 1 d R . . 
C11 C 0.2364(3) 0.05878(18) 0.41713(10) 0.0161(4) Uani 1 1 d . . . 
H11 H 0.2708 0.1104 0.4491 0.019 Uiso 1 1 d R . . 
O12 O 0.1224(2) 0.12066(14) 0.37283(8) 0.0178(3) Uani 1 1 d . . . 
O13 O 0.2950(3) -0.16466(16) 0.57314(9) 0.0273(4) Uani 1 1 d . . . 
C14 C 0.1710(4) -0.1586(2) 0.41778(12) 0.0222(5) Uani 1 1 d . . . 
H14 H 0.0826 -0.1987 0.3902 0.027 Uiso 1 1 d R . . 
C15 C 0.1998(4) 0.2223(2) 0.25892(11) 0.0214(5) Uani 1 1 d . . . 
C16 C 0.2647(5) 0.3328(2) 0.22611(13) 0.0324(6) Uani 1 1 d . . . 
H16A H 0.2381 0.3242 0.1842 0.049 Uiso 1 1 d R . . 
H16B H 0.1857 0.3965 0.2413 0.049 Uiso 1 1 d R . . 
H16C H 0.4102 0.3469 0.2323 0.049 Uiso 1 1 d R . . 
C17 C -0.0275(4) 0.1943(3) 0.24525(13) 0.0317(6) Uani 1 1 d . . . 
H17A H -0.0476 0.1896 0.2029 0.048 Uiso 1 1 d R . . 
H17B H -0.0635 0.1220 0.2632 0.048 Uiso 1 1 d R . . 
H17C H -0.1145 0.2539 0.2613 0.048 Uiso 1 1 d R . . 
C18 C 0.3368(5) 0.1241(3) 0.23445(13) 0.0348(7) Uani 1 1 d . . . 
H18A H 0.3156 0.1169 0.1922 0.052 Uiso 1 1 d R . . 
H18B H 0.4803 0.1410 0.2422 0.052 Uiso 1 1 d R . . 
H18C H 0.2997 0.0532 0.2537 0.052 Uiso 1 1 d R . . 
C19 C 0.1670(4) 0.3686(2) 0.38111(12) 0.0223(5) Uani 1 1 d . . . 
C20 C 0.3091(4) 0.4704(2) 0.36547(14) 0.0301(6) Uani 1 1 d . . . 
H20A H 0.2622 0.5377 0.3863 0.045 Uiso 1 1 d R . . 
H20B H 0.4496 0.4533 0.3769 0.045 Uiso 1 1 d R . . 
H20C H 0.3035 0.4840 0.3232 0.045 Uiso 1 1 d R . . 
C21 C -0.0594(5) 0.3996(2) 0.36352(16) 0.0351(7) Uani 1 1 d . . . 
H21A H -0.1001 0.4694 0.3832 0.053 Uiso 1 1 d R . . 
H21B H -0.0675 0.4100 0.3211 0.053 Uiso 1 1 d R . . 
H21C H -0.1507 0.3384 0.3753 0.053 Uiso 1 1 d R . . 
C22 C 0.1765(6) 0.3501(2) 0.44879(13) 0.0392(8) Uani 1 1 d . . . 
H22A H 0.1352 0.4194 0.4689 0.059 Uiso 1 1 d R . . 
H22B H 0.0836 0.2888 0.4595 0.059 Uiso 1 1 d R . . 
H22C H 0.3156 0.3302 0.4604 0.059 Uiso 1 1 d R . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
SI1 O2 1.6465(16) . ? 
SI1 O12 1.6696(16) . ? 
SI1 C19 1.877(2) . ? 
SI1 C15 1.901(3) . ? 
O2 C3 1.427(3) . ? 
C3 C4 1.518(3) . ? 
C3 H3A 0.9599 . ? 
C3 H3B 0.9600 . ? 
C4 O5 1.443(3) . ? 
C4 C11 1.525(3) . ? 
C4 H4 0.9600 . ? 
O5 C6 1.413(3) . ? 
C6 C14 1.486(4) . ? 
C6 C7 1.507(4) . ? 
C6 H6 0.9600 . ? 
C7 C8 1.486(4) . ? 
C7 C14 1.515(3) . ? 
C7 H7 0.9599 . ? 
C8 O13 1.203(3) . ? 
C8 O9 1.359(3) . ? 
O9 C10 1.452(3) . ? 
C10 C14 1.517(3) . ? 
C10 C11 1.539(3) . ? 
C10 H10 0.9600 . ? 
C11 O12 1.428(3) . ? 
C11 H11 0.9599 . ? 
C14 H14 0.9599 . ? 
C15 C17 1.529(3) . ? 
C15 C16 1.538(4) . ? 
C15 C18 1.542(4) . ? 
C16 H16A 0.9600 . ? 
C16 H16B 0.9600 . ? 
C16 H16C 0.9600 . ? 
C17 H17A 0.9600 . ? 
C17 H17B 0.9600 . ? 
C17 H17C 0.9601 . ? 
C18 H18A 0.9604 . ? 
C18 H18B 0.9600 . ? 
C18 H18C 0.9599 . ? 
C19 C22 1.533(4) . ? 
C19 C20 1.536(3) . ? 
C19 C21 1.551(4) . ? 
C20 H20A 0.9601 . ? 
C20 H20B 0.9600 . ? 
C20 H20C 0.9600 . ? 
C21 H21A 0.9601 . ? 
C21 H21B 0.9600 . ? 
C21 H21C 0.9600 . ? 
C22 H22A 0.9600 . ? 
C22 H22B 0.9600 . ? 
C22 H22C 0.9600 . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O2 SI1 O12 105.81(9) . . ? 
O2 SI1 C19 107.47(11) . . ? 
O12 SI1 C19 109.66(10) . . ? 
O2 SI1 C15 109.85(10) . . ? 
O12 SI1 C15 106.03(10) . . ? 
C19 SI1 C15 117.45(11) . . ? 
C3 O2 SI1 128.57(14) . . ? 
O2 C3 C4 110.20(18) . . ? 
O2 C3 H3A 110.0 . . ? 
C4 C3 H3A 109.6 . . ? 
O2 C3 H3B 109.3 . . ? 
C4 C3 H3B 109.4 . . ? 
H3A C3 H3B 108.2 . . ? 
O5 C4 C3 109.86(19) . . ? 
O5 C4 C11 109.14(18) . . ? 
C3 C4 C11 110.76(19) . . ? 
O5 C4 H4 109.0 . . ? 
C3 C4 H4 109.3 . . ? 
C11 C4 H4 108.7 . . ? 
C6 O5 C4 107.77(18) . . ? 
O5 C6 C14 117.2(2) . . ? 
O5 C6 C7 119.8(2) . . ? 
C14 C6 C7 60.79(17) . . ? 
O5 C6 H6 115.6 . . ? 
C14 C6 H6 116.0 . . ? 
C7 C6 H6 116.3 . . ? 
C8 C7 C6 117.5(2) . . ? 
C8 C7 C14 105.8(2) . . ? 
C6 C7 C14 58.94(16) . . ? 
C8 C7 H7 119.1 . . ? 
C6 C7 H7 120.0 . . ? 
C14 C7 H7 119.3 . . ? 
O13 C8 O9 120.9(2) . . ? 
O13 C8 C7 128.8(2) . . ? 
O9 C8 C7 110.2(2) . . ? 
C8 O9 C10 111.81(19) . . ? 
O9 C10 C14 106.28(19) . . ? 
O9 C10 C11 106.52(18) . . ? 
C14 C10 C11 113.89(19) . . ? 
O9 C10 H10 109.9 . . ? 
C14 C10 H10 109.9 . . ? 
C11 C10 H10 110.2 . . ? 
O12 C11 C4 108.10(17) . . ? 
O12 C11 C10 111.69(17) . . ? 
C4 C11 C10 110.68(18) . . ? 
O12 C11 H11 108.8 . . ? 
C4 C11 H11 108.8 . . ? 
C10 C11 H11 108.7 . . ? 
C11 O12 SI1 115.28(13) . . ? 
C6 C14 C7 60.27(17) . . ? 
C6 C14 C10 111.6(2) . . ? 
C7 C14 C10 105.4(2) . . ? 
C6 C14 H14 121.7 . . ? 
C7 C14 H14 121.2 . . ? 
C10 C14 H14 121.0 . . ? 
C17 C15 C16 110.0(2) . . ? 
C17 C15 C18 108.5(2) . . ? 
C16 C15 C18 107.1(2) . . ? 
C17 C15 SI1 111.33(18) . . ? 
C16 C15 SI1 112.11(18) . . ? 
C18 C15 SI1 107.69(17) . . ? 
C15 C16 H16A 109.4 . . ? 
C15 C16 H16B 109.3 . . ? 
H16A C16 H16B 109.5 . . ? 
C15 C16 H16C 109.7 . . ? 
H16A C16 H16C 109.5 . . ? 
H16B C16 H16C 109.5 . . ? 
C15 C17 H17A 109.8 . . ? 
C15 C17 H17B 109.4 . . ? 
H17A C17 H17B 109.5 . . ? 
C15 C17 H17C 109.2 . . ? 
H17A C17 H17C 109.5 . . ? 
H17B C17 H17C 109.5 . . ? 
C15 C18 H18A 109.5 . . ? 
C15 C18 H18B 109.4 . . ? 
H18A C18 H18B 109.5 . . ? 
C15 C18 H18C 109.5 . . ? 
H18A C18 H18C 109.5 . . ? 
H18B C18 H18C 109.5 . . ? 
C22 C19 C20 108.1(2) . . ? 
C22 C19 C21 108.7(3) . . ? 
C20 C19 C21 108.7(2) . . ? 
C22 C19 SI1 109.04(17) . . ? 
C20 C19 SI1 112.45(18) . . ? 
C21 C19 SI1 109.72(19) . . ? 
C19 C20 H20A 109.3 . . ? 
C19 C20 H20B 109.9 . . ? 
H20A C20 H20B 109.5 . . ? 
C19 C20 H20C 109.3 . . ? 
H20A C20 H20C 109.5 . . ? 
H20B C20 H20C 109.5 . . ? 
C19 C21 H21A 109.7 . . ? 
C19 C21 H21B 109.4 . . ? 
H21A C21 H21B 109.5 . . ? 
C19 C21 H21C 109.4 . . ? 
H21A C21 H21C 109.5 . . ? 
H21B C21 H21C 109.5 . . ? 
C19 C22 H22A 109.6 . . ? 
C19 C22 H22B 109.1 . . ? 
H22A C22 H22B 109.5 . . ? 
C19 C22 H22C 109.8 . . ? 
H22A C22 H22C 109.5 . . ? 
H22B C22 H22C 109.5 . . ? 
 
_diffrn_measured_fraction_theta_max    0.995 
_diffrn_reflns_theta_full              27.50 
_diffrn_measured_fraction_theta_full   0.995 
_refine_diff_density_max    0.914 
_refine_diff_density_min   -0.501 
_refine_diff_density_rms    0.088 
#===END
